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Multistage pore ZSM-5 catalyst for preparing acrolein by glycerol dehydration and preparation method of catalyst

A ZSM-5 catalyst technology, applied in the field of multi-stage molecular sieve catalyst and its preparation, to achieve high selectivity, suitable for large-scale production, and high practical value

Inactive Publication Date: 2016-06-01
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Multistage pore ZSM-5 catalyst for preparing acrolein by glycerol dehydration and preparation method of catalyst
  • Multistage pore ZSM-5 catalyst for preparing acrolein by glycerol dehydration and preparation method of catalyst
  • Multistage pore ZSM-5 catalyst for preparing acrolein by glycerol dehydration and preparation method of catalyst

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Embodiment 1

[0031] (a) Take the silicon source as sodium silicate crystal, the aluminum source as sodium metaaluminate, the template agent as tetrapropylammonium bromide and deionized water, and weigh each material according to the molar ratio, that is, SiO 2 :Al 2 o 3 : Templating agent: H 2 O=1:0.0025:0.3:30, one-step feeding to prepare a mixed solution; heat the mixed solution to 80°C for ultrasonic dissolution, ultrasonic frequency 40KHZ, wait for 10 minutes of ultrasonication, then immediately lower the temperature to 40°C quickly, add After a certain amount of ethanol (ethanol / Si=0.1), then quickly add sulfuric acid dropwise under stirring (stirring speed: 180r / min) to adjust the pH to 8-10 to form a gel;

[0032] (b) Stir the obtained gel for 48 hours at a rotation speed of 250r / min, and control the ambient temperature at 40°C while stirring;

[0033] (c) Transfer the obtained precursor into an autoclave for crystallization at 180 °C for 48 h. After crystallization, cool and fi...

Embodiment 2

[0037] (a) Take the silicon source as tetraethyl orthosilicate, the aluminum source as aluminum nitrate, the template agent as tetrapropylammonium hydroxide and deionized water, and weigh each material according to the molar ratio, that is, SiO 2 :Al 2 o 3 : Templating agent: H 2 O=1:0.0025:0.1:40, one-step feeding to prepare a mixed solution; heat the mixed solution to 70°C for ultrasonic dissolution, the ultrasonic frequency is 80KHZ, wait for 15 minutes of ultrasonication, then immediately reduce the temperature to 40°C quickly, add After a certain amount of ethanol (ethanol / Si=0.2), then quickly add sulfuric acid dropwise under stirring (stirring speed: 200r / min) to adjust the pH to 8-10 to form a gel;

[0038] (b) Stir the obtained gel for 24 hours at a rotational speed of 350r / min, and control the ambient temperature at 40°C while stirring;

[0039] (c) Transfer the obtained precursor into an autoclave for crystallization at 150 °C for 60 h. After crystallization, co...

Embodiment 3

[0043] (a) Take silicon source as white carbon black, aluminum source as aluminum sulfate, template agent as tetrapropylammonium bromide and deionized water, and weigh each substance according to the molar ratio, that is, SiO 2 :Al 2 o 3 : Templating agent: H 2 O=1:0.002:0.2:60, one-step feeding to prepare a mixed solution; heat the mixed solution to 75°C for ultrasonic dissolution, ultrasonic frequency 50KHZ, wait for 10 minutes of ultrasonication, then immediately lower the temperature to 40°C quickly, add After a certain amount of ethanol (ethanol / Si=0.1), then quickly add sulfuric acid dropwise under stirring (stirring speed: 200r / min) to adjust the pH to 8-10 to form a gel;

[0044] (b) The obtained gel was stirred for 40 hours at a rotation speed of 300r / min, and the ambient temperature was controlled at 40°C during stirring;

[0045] (c) Transfer the obtained precursor into an autoclave for crystallization at 170 °C for 55 h. After crystallization, cool and filter, ...

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Abstract

The invention belongs to the technical field of chemical catalysts and particularly relates to a multistage pore ZSM-5 catalyst for preparing acrolein by glycerol dehydration and a preparation method of the catalyst. The catalyst comprises a multistage pore ZSM-5 molecular sieve which comprises rich transgranular mesopores; the preparation method comprises the steps that cheap silicon source, aluminium source and organic template reagent are dissolved in water, cavatition of ultrasonic wave and fierce mechanical agitation are used, few small molecular alcohol is added as a cosolvent, and a multistage pore ZSM-5 molecular sieve with MFI structure property is synthesized with a hydrothermal method. The multistage pore ZSM-5 molecular sieve which comprises rich transgranular mesopores is obtained through the cheap preparation technology, the crystal grain is large, the hydrothermal stability is good, and high selectivity and high stability are shown in the acrolein preparation process by glycerol dehydration.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysts, and in particular relates to a hierarchical porous molecular sieve catalyst for catalyzing the dehydration of glycerin to prepare acrolein and a preparation method thereof. Background technique [0002] Due to the increasing scarcity of traditional fossil resources, the energy crisis has become an important issue plaguing the world, and researchers are devoting themselves to the development of renewable energy. Among them, biodiesel (triglyceride) has been widely used due to its advantages of environmental protection and renewability. With the increase of biodiesel production, the supply of its main by-product glycerol has also exceeded the demand. Therefore, it has become a research hotspot in the world to find new ways to utilize the cheap and abundant glycerol. [0003] Among the multiple utilization pathways of glycerol, the conversion to acrolein through dehydration reaction is ...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J29/40C07C47/22C07C45/52
CPCC01B39/40C07C45/52B01J29/40C01P2002/72C01P2004/04B01J35/647C07C47/22
Inventor 沈伟黄亮徐华龙胡志洁王圣庄思爽秦枫
Owner FUDAN UNIV
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